CN111978220A - Method for synthesizing clethodim crude drug - Google Patents
Method for synthesizing clethodim crude drug Download PDFInfo
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- CN111978220A CN111978220A CN202010797927.8A CN202010797927A CN111978220A CN 111978220 A CN111978220 A CN 111978220A CN 202010797927 A CN202010797927 A CN 202010797927A CN 111978220 A CN111978220 A CN 111978220A
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- Prior art keywords
- wastewater
- tank
- petroleum ether
- pump
- kettle
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- 239000003814 drug Substances 0.000 title claims abstract description 23
- 229940079593 drug Drugs 0.000 title claims abstract description 23
- 239000005497 Clethodim Substances 0.000 title claims abstract description 18
- SILSDTWXNBZOGF-JWGBMQLESA-N clethodim Chemical compound CCSC(C)CC1CC(O)=C(C(CC)=NOC\C=C\Cl)C(=O)C1 SILSDTWXNBZOGF-JWGBMQLESA-N 0.000 title claims abstract description 18
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000002351 wastewater Substances 0.000 claims abstract description 46
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003208 petroleum Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 26
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 26
- 238000005086 pumping Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- VOYADQIFGGIKAT-UHFFFAOYSA-N 1,3-dibutyl-4-hydroxy-2,6-dioxopyrimidine-5-carboximidamide Chemical compound CCCCn1c(O)c(C(N)=N)c(=O)n(CCCC)c1=O VOYADQIFGGIKAT-UHFFFAOYSA-N 0.000 claims abstract description 5
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000110 cooling liquid Substances 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 12
- 229920002994 synthetic fiber Polymers 0.000 claims description 8
- 239000008399 tap water Substances 0.000 claims description 8
- 235000020679 tap water Nutrition 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 238000007790 scraping Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims 2
- 239000002912 waste gas Substances 0.000 abstract description 3
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/14—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides
- C07C319/20—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides by reactions not involving the formation of sulfide groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for synthesizing clethodim crude drug, which is characterized by comprising the following steps: s1, pumping petroleum ether into a synthesis kettle; s2, injecting the trione into a synthesis kettle at one time; s3, injecting chloramine into a synthesis kettle at one time; s4, draining jacket condensate water; s5, adding hydrochloric acid into the hydrochloric acid meter; s6, dropwise adding hydrochloric acid into the synthesis kettle, and distributing the lower-layer wastewater into a wastewater tank; s7, dividing the lower layer wastewater into wastewater tanks; s8, separating the lower layer wastewater into wastewater tanks again; s9, dividing the washed synthetic liquid petroleum ether material into synthetic liquid tanks; s10, desolventizing; s11, carrying out continuous scraper film desolventizing operation; s12, introducing nitrogen to break vacuum; s13, closing a cooling liquid valve of the main cooler; s14, throwing the removed petroleum ether into an intermediate tank to synthesize the petroleum ether; and S15, discharging the crude drug from the receiving tank. The invention has the advantages that: the waste water and gas generation amount is small, the subsequent treatment is convenient, the monitoring data amount is small, and the control is convenient.
Description
Technical Field
The invention relates to the technical field of clethodim, in particular to a method for synthesizing crude clethodim technical.
Background
The clethodim is a stem leaf herbicide, is an efficient, safe and high-selectivity ACCase inhibitor, has special effect on most annual and perennial gramineous weeds, and is safe to dicotyledonous crops. The clethodim finished product is obtained by refining a clethodim crude drug, but the existing synthesis method of the clethodim crude drug generates a large amount of waste gas and waste water in the synthesis process, so that the subsequent treatment cost is high; meanwhile, the existing clethodim crude drug synthesis method needs to monitor a large amount of data at the same time and is not easy to control.
Disclosure of Invention
The invention aims to solve the technical problem of providing a clethodim crude drug synthesis method which is low in waste water and waste gas generation amount, convenient for subsequent treatment, low in monitoring data amount and convenient to control.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method for synthesizing clethodim crude drug comprises the following steps:
s1, starting a synthetic petroleum ether pump in the middle tank area to pump 2100L petroleum ether into the synthetic kettle at one time;
s2, pumping the one-time metered fine trione into a synthesis kettle at one time through a pump;
s3, pumping the barreled and metered chloramine into a synthesis kettle at one time through a pump;
s4, draining off condensed water in a jacket of the synthesis kettle, slightly opening a jacket steam valve, slowly heating the material to 60 ℃ within 2 hours, keeping the temperature for 4 hours at the temperature, closing the jacket steam valve after the time is qualified in sampling analysis, draining off the jacket condensed water, arranging a remote thermometer in the synthesis kettle, and interlocking with a steam feed cut-off valve;
s5, starting a hydrochloric acid pump in the middle tank area, and pumping 500L of hydrochloric acid into the hydrochloric acid metering tank;
s6, dropwise adding hydrochloric acid into the synthesis kettle, adjusting the pH value of the feed liquid to 1-2, stirring for 15min, standing for 20min, repeatedly measuring the pH value unchanged, distributing the lower-layer wastewater into a wastewater tank, and conveying the lower-layer wastewater to the wastewater pH value adjustment kettle through a wastewater pump;
s7, adding 1400L of washing synthetic material into the kettle through a tap water electronic flowmeter for washing, stirring for 15min, standing for 20min, and completely discharging lower-layer wastewater into a wastewater tank;
s8, adding 1400L of washing synthetic material into the kettle again through a tap water electronic flowmeter for washing, stirring for 15min, standing for 20min, and completely discharging lower-layer wastewater into a wastewater tank;
s9, dividing the washed synthetic liquid petroleum ether material into synthetic liquid tanks;
s10, adjusting the temperature of the hot water tank to 80 ℃, starting a desolventizing vacuum pump, starting a hot water pump, and opening a feed valve of a preheater to perform desolventizing operation;
s11, adjusting the flow rate, controlling the water temperature and the vacuum degree, and performing continuous film-scraping and desolventizing operation;
s12, stopping a preheater feeding valve and a heat-stopping water pump, idling for 5min, stopping a vacuum system when no material comes out, and starting the system to feed nitrogen and break vacuum;
s13, closing a cooling liquid valve of the main cooler;
s14, enabling the separated petroleum ether to enter a receiving tank and transfer into a petroleum ether receiving tank of a main tank, and pumping the petroleum ether into a petroleum ether synthesizing tank of an intermediate tank through a petroleum ether pump;
and S15, discharging the crude drug from the receiving tank, and packaging the crude drug.
Further, the petroleum ether in S1 was weighed by an electronic flowmeter.
Furthermore, the water temperature in the S11 is 80 ℃, and the vacuum degree is-0.098 Mpa.
Compared with the prior art, the invention has the advantages that: according to the method for synthesizing the clethodim crude drug, only wastewater is generated in the synthesis process, the subsequent treatment is convenient, the treatment cost is effectively reduced, and the harm to the environment is reduced; a large amount of data does not need to be monitored, synthetic control is facilitated, and misoperation and safety accidents are avoided.
Detailed Description
Example one
A method for synthesizing clethodim crude drug comprises the following steps:
s1, starting a synthetic petroleum ether pump in the middle tank area to pump 2100L petroleum ether into a synthetic kettle at one time through an electronic flowmeter;
s2, pumping the one-time metered fine trione into a synthesis kettle at one time through a pump;
s3, pumping the barreled and metered chloramine into a synthesis kettle at one time through a pump;
s4, draining off condensed water in a jacket of the synthesis kettle, slightly opening a jacket steam valve, slowly heating the material to 60 ℃ within 2 hours, keeping the temperature for 4 hours at the temperature, closing the jacket steam valve after the time is qualified in sampling analysis, draining off the jacket condensed water, arranging a remote thermometer in the synthesis kettle, and interlocking with a steam feed cut-off valve;
s5, starting a hydrochloric acid pump in the middle tank area, and pumping 500L of hydrochloric acid into the hydrochloric acid metering tank;
s6, dropwise adding hydrochloric acid into the synthesis kettle, adjusting the pH value of the feed liquid to 1.5, stirring for 15min, standing for 20min, repeatedly measuring the pH value unchanged, distributing the lower-layer wastewater into a wastewater tank, and conveying the lower-layer wastewater to the wastewater pH value adjustment kettle through a wastewater pump;
s7, adding 1400L of washing synthetic material into the kettle through a tap water electronic flowmeter for washing, stirring for 15min, standing for 20min, and completely discharging lower-layer wastewater into a wastewater tank;
s8, adding 1400L of washing synthetic material into the kettle again through a tap water electronic flowmeter for washing, stirring for 15min, standing for 20min, and completely discharging lower-layer wastewater into a wastewater tank;
s9, dividing the washed synthetic liquid petroleum ether material into synthetic liquid tanks;
s10, adjusting the temperature of the hot water tank to 80 ℃, starting a desolventizing vacuum pump, starting a hot water pump, and opening a feed valve of a preheater to perform desolventizing operation;
s11, adjusting the flow rate, controlling the water temperature to 80 ℃ and the vacuum degree to-0.098 Mpa, and performing continuous film-scraping and desolventizing operation;
s12, stopping a preheater feeding valve and a heat-stopping water pump, idling for 5min, stopping a vacuum system when no material comes out, and starting the system to feed nitrogen and break vacuum;
s13, closing a cooling liquid valve of the main cooler;
s14, enabling the separated petroleum ether to enter a receiving tank and transfer into a petroleum ether receiving tank of a main tank, and pumping the petroleum ether into a petroleum ether synthesizing tank of an intermediate tank through a petroleum ether pump;
and S15, discharging the crude drug from the receiving tank, and packaging the crude drug.
Example two
A method for synthesizing clethodim crude drug comprises the following steps:
s1, starting a synthetic petroleum ether pump in the middle tank area to pump 2100L petroleum ether into a synthetic kettle at one time through an electronic flowmeter;
s2, pumping the one-time metered fine trione into a synthesis kettle at one time through a pump;
s3, pumping the barreled and metered chloramine into a synthesis kettle at one time through a pump;
s4, draining off condensed water in a jacket of the synthesis kettle, slightly opening a jacket steam valve, slowly heating the material to 60 ℃ within 1.8 hours, keeping the temperature for 4 hours at the temperature, closing the jacket steam valve after sampling and analyzing are qualified, draining off the jacket condensed water, arranging a remote thermometer in the synthesis kettle, and interlocking with a steam feed cut-off valve;
s5, starting a hydrochloric acid pump in the middle tank area, and pumping 500L of hydrochloric acid into the hydrochloric acid metering tank;
s6, dropwise adding hydrochloric acid into the synthesis kettle, adjusting the pH value of the feed liquid to 1.8, stirring for 15min, standing for 20min, repeatedly measuring the pH value unchanged, distributing the lower-layer wastewater into a wastewater tank, and conveying the lower-layer wastewater to the wastewater pH value adjustment kettle through a wastewater pump;
s7, adding 1400L of washing synthetic material into the kettle through a tap water electronic flowmeter for washing, stirring for 15min, standing for 20min, and completely discharging lower-layer wastewater into a wastewater tank;
s8, adding 1400L of washing synthetic material into the kettle again through a tap water electronic flowmeter for washing, stirring for 15min, standing for 20min, and completely discharging lower-layer wastewater into a wastewater tank;
s9, dividing the washed synthetic liquid petroleum ether material into synthetic liquid tanks;
s10, adjusting the temperature of the hot water tank to 80 ℃, starting a desolventizing vacuum pump, starting a hot water pump, and opening a feed valve of a preheater to perform desolventizing operation;
s11, adjusting the flow rate, controlling the water temperature to 80 ℃ and the vacuum degree to-0.098 Mpa, and performing continuous film-scraping and desolventizing operation;
s12, stopping a preheater feeding valve and a heat-stopping water pump, idling for 5min, stopping a vacuum system when no material comes out, and starting the system to feed nitrogen and break vacuum;
s13, closing a cooling liquid valve of the main cooler;
s14, enabling the separated petroleum ether to enter a receiving tank and transfer into a petroleum ether receiving tank of a main tank, and pumping the petroleum ether into a petroleum ether synthesizing tank of an intermediate tank through a petroleum ether pump;
and S15, discharging the crude drug from the receiving tank, and packaging the crude drug.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (3)
1. A method for synthesizing clethodim crude drug is characterized by comprising the following steps:
s1, starting a synthetic petroleum ether pump in the middle tank area to pump 2100L petroleum ether into the synthetic kettle at one time;
s2, pumping the one-time metered fine trione into a synthesis kettle at one time through a pump;
s3, pumping the barreled and metered chloramine into a synthesis kettle at one time through a pump;
s4, draining off condensed water in a jacket of the synthesis kettle, slightly opening a jacket steam valve, slowly heating the material to 60 ℃ within 2 hours, keeping the temperature for 4 hours at the temperature, closing the jacket steam valve after the time is qualified in sampling analysis, draining off the jacket condensed water, arranging a remote thermometer in the synthesis kettle, and interlocking with a steam feed cut-off valve;
s5, starting a hydrochloric acid pump in the middle tank area, and pumping 500L of hydrochloric acid into the hydrochloric acid metering tank;
s6, dropwise adding hydrochloric acid into the synthesis kettle, adjusting the pH value of the feed liquid to 1-2, stirring for 15min, standing for 20min, repeatedly measuring the pH value unchanged, distributing the lower-layer wastewater into a wastewater tank, and conveying the lower-layer wastewater to the wastewater pH value adjustment kettle through a wastewater pump;
s7, adding 1400L of washing synthetic material into the kettle through a tap water electronic flowmeter for washing, stirring for 15min, standing for 20min, and completely discharging lower-layer wastewater into a wastewater tank;
s8, adding 1400L of washing synthetic material into the kettle again through a tap water electronic flowmeter for washing, stirring for 15min, standing for 20min, and completely discharging lower-layer wastewater into a wastewater tank;
s9, dividing the washed synthetic liquid petroleum ether material into synthetic liquid tanks;
s10, adjusting the temperature of the hot water tank to 80 ℃, starting a desolventizing vacuum pump, starting a hot water pump, and opening a feed valve of a preheater to perform desolventizing operation;
s11, adjusting the flow rate, controlling the water temperature and the vacuum degree, and performing continuous film-scraping and desolventizing operation;
s12, stopping a preheater feeding valve and a heat-stopping water pump, idling for 5min, stopping a vacuum system when no material comes out, and starting the system to feed nitrogen and break vacuum;
s13, closing a cooling liquid valve of the main cooler;
s14, enabling the separated petroleum ether to enter a receiving tank and transfer into a petroleum ether receiving tank of a main tank, and pumping the petroleum ether into a petroleum ether synthesizing tank of an intermediate tank through a petroleum ether pump;
and S15, discharging the crude drug from the receiving tank, and packaging the crude drug.
2. The method for synthesizing clethodim crude drug compound according to claim 1, characterized in that: the petroleum ether in S1 was weighed by an electronic flow meter.
3. The method for synthesizing clethodim crude drug compound according to claim 1, characterized in that: the water temperature in the S11 is 80 ℃, and the vacuum degree is-0.098 Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010797927.8A CN111978220A (en) | 2020-08-10 | 2020-08-10 | Method for synthesizing clethodim crude drug |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010797927.8A CN111978220A (en) | 2020-08-10 | 2020-08-10 | Method for synthesizing clethodim crude drug |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111978220A true CN111978220A (en) | 2020-11-24 |
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| CN202010797927.8A Pending CN111978220A (en) | 2020-08-10 | 2020-08-10 | Method for synthesizing clethodim crude drug |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013007054A1 (en) * | 2011-07-08 | 2013-01-17 | Ningbo Ocean Chemical New Materials Technology Co., Ltd. | Method for preparation of ketoxime compound and method for preparation of alkoxy-amine hydrochloride |
| CN105418470A (en) * | 2015-11-17 | 2016-03-23 | 江苏长青农化股份有限公司 | Synthetic method of clethodim |
| CN106187841A (en) * | 2016-07-08 | 2016-12-07 | 山东润博生物科技有限公司 | A kind of industrialized process for preparing of clethodim |
| CN111087333A (en) * | 2019-12-24 | 2020-05-01 | 江苏长青农化股份有限公司 | Method for preparing clethodim technical through low-temperature condensation |
-
2020
- 2020-08-10 CN CN202010797927.8A patent/CN111978220A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013007054A1 (en) * | 2011-07-08 | 2013-01-17 | Ningbo Ocean Chemical New Materials Technology Co., Ltd. | Method for preparation of ketoxime compound and method for preparation of alkoxy-amine hydrochloride |
| CN105418470A (en) * | 2015-11-17 | 2016-03-23 | 江苏长青农化股份有限公司 | Synthetic method of clethodim |
| CN106187841A (en) * | 2016-07-08 | 2016-12-07 | 山东润博生物科技有限公司 | A kind of industrialized process for preparing of clethodim |
| CN111087333A (en) * | 2019-12-24 | 2020-05-01 | 江苏长青农化股份有限公司 | Method for preparing clethodim technical through low-temperature condensation |
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Application publication date: 20201124 |
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